WO2021211231A2 - Électrodes de métal de transition revêtues de carbone pour réacteurs d'oxydation avancée - Google Patents

Électrodes de métal de transition revêtues de carbone pour réacteurs d'oxydation avancée Download PDF

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WO2021211231A2
WO2021211231A2 PCT/US2021/021739 US2021021739W WO2021211231A2 WO 2021211231 A2 WO2021211231 A2 WO 2021211231A2 US 2021021739 W US2021021739 W US 2021021739W WO 2021211231 A2 WO2021211231 A2 WO 2021211231A2
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cathode
advanced oxidation
reactor
reactor vessel
ozone
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PCT/US2021/021739
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WO2021211231A3 (fr
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Ramya Srinivasan
Indumathi Nambi
Prakash Govindan
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Gradiant Corporation
Indian Institute Of Technology
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Publication of WO2021211231A2 publication Critical patent/WO2021211231A2/fr
Publication of WO2021211231A3 publication Critical patent/WO2021211231A3/fr

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  • Electrodes for advanced oxidation reactors and related methods are generally described.
  • Advanced oxidation processes offer a solution to these difficult contaminants. Such processes produce hydroxyl radicals and other powerful oxidants capable of breaking almost any organic bond. Thus, organic pollutants that cannot be removed by conventional treatment can typically be removed by these techniques. Advanced oxidation, however, is still an emerging technology and is not yet fully adapted to industrial scales. Many advanced oxidation processes require the storage of dangerous chemicals, and many more are inefficient and energy-intensive.
  • hydroxyl radicals are generated by reacting ozone with hydrogen peroxide, wherein the hydrogen peroxide is electrochemically produced in situ with a cathode.
  • the required ozone may be produced in an electrical ozone generator, allowing all reactants to be generated on-site, removing chemical storage requirements.
  • the process can be practiced at a wide pH range.
  • a cathode for an advanced oxidation reactor and a method for advanced oxidation are described herein, where various embodiments of the apparatus and methods may include some or all of the elements, features, and steps described below.
  • the cathode can include a transition-metal foam and a carbon coating on the transition-metal foam.
  • the advanced oxidation reactor includes the cathode and an anode configured and positioned relative to the cathode so as to enable a potential difference to be applied across the anode and the cathode.
  • the cathode is used to produce hydrogen peroxide for reaction with ozone to produce hydroxyl radicals in the electroperoxone process.
  • a cathode comprising a transition-metal foam and a carbon coating on the transition-metal foam is electrified to produce an electrified cathode.
  • the electrified cathode is used to produce a hydrogen-peroxide product via a first electrochemical reaction.
  • the hydrogen peroxide product is then used in a second electrochemical reaction to produce OH radicals.
  • Organic molecules are then oxidized from a feed stream using the OH radicals.
  • a provided cathode and an anode are electrically connectable to a source of direct current, and the cathode and anode are at least partially submerged in a liquid bath comprising a feed solution in a reactor vessel.
  • the cathode comprises a carbon-coated nickel foam.
  • a gas stream comprising ozone is injected into the liquid bath.
  • a gas stream comprising oxygen is injected into the liquid bath.
  • a current is transmitted from the cathode to the anode, resulting in an electrochemical reaction in which hydroxyl radicals are produced.
  • Organic chemicals contained in the liquid bath are oxidized by the hydroxyl radicals.
  • FIG. 1 is a schematic diagram of an exemplary advanced oxidation reactor 100 configured to produce hydroxyl radicals using an electroperoxone process.
  • FIG. 2 is a schematic diagram of an electrode 101/ 103.
  • first, second, third, etc. maybe used herein to describe various elements, these elements are not to be limited by these terms. These terms are simply used to distinguish one element from another. Thus, a first element, discussed below, could be termed a second element without departing from the teachings of the exemplary embodiments. In addition, where a range of values is provided, each subrange and each individual value between the upper and lower ends of the range is contemplated and therefore disclosed.
  • the various components identified herein can be provided in an assembled and finished form; or some or all of the components can be packaged together and marketed as a kit with instructions (e.g., in written, video or audio form) for assembly and/or modification by a customer to produce a finished product.
  • Carbon-coated transition-metal electrodes for advanced oxidation reactors and related systems and methods are generally described herein. According to various exemplifications, organic constituents of a feed stream can be oxidized and/ or mineralized by advanced oxidation in a reactor with the carbon-coated transition-metal electrode.
  • Advanced oxidation processes comprise the production of hydroxyl radicals and/ or other oxidants that can be used to break bonds in organic molecules.
  • the hydroxyl radical is a relatively powerful oxidant due to its high oxidation potential and its capability of breaking most types of organic bonds.
  • the hydroxyl radical is often called a nonspecific oxidant. Due to this advantage, the advanced oxidation processes can be beneficial in treating persistent organic species that are resistant to typical oxidation processes, as well as being resistant to natural degradation, such as those species found in landfill leachate, pharmaceutical wastewater, and oilfield wastewater.
  • Various exemplifications include an advanced oxidation reactor configured to produce hydroxyl radicals.
  • the hydroxyl radicals produced by the process can be used to oxidize and/or mineralize organic species.
  • mineralization refers to the complete oxidation of an organic molecule, wherein the remnants of the oxidized molecule can consist solely of carbon dioxide, water, and other inorganic molecules.
  • the advanced oxidation reactor includes one or more electrodes that, according to various exemplifications, can be disposed within a reactor vessel.
  • the reactor vessel can further include one or more gas inlets fluidically connected to a source of ozone and/or a source of oxygen.
  • the advanced oxidation reactor can be configured for an electroperoxone process.
  • FIG. 1 is a schematic diagram of an exemplary advanced oxidation reactor 100, configured to produce hydroxyl radicals using the electroperoxone process.
  • the advanced oxidation reactor 100 includes one or more electrodes 101 and 103.
  • the advanced oxidation reactor 100 includes a first electrode 101 and a second electrode 103.
  • the one or more electrodes 101/ 103 can be selected from cathodes and/ or anodes.
  • a cathode is an electrode configured to facilitate electrochemical reduction reactions.
  • the cathode can be electrically connectable to a negative terminal of a direct-current power source, such that negatively charged electrons can flow from the current source to the electrode.
  • the first electrode 101 in an advanced oxidation reactor 100 is a cathode electrically connected to the negative (-) terminal of a direct-current power source 105 such that electrons can flow from the source 105 to the cathode 101.
  • an anode is an electrode that is configured to facilitate electrochemical oxidation reactions.
  • the anode can be electrically connectable to a positive terminal of a direct-current power source, such that electrons can flow from the electrode to the source of current.
  • the second electrode 103 in the advanced oxidation reactor 100 is an anode and is electrically connected to the positive (+) terminal of the direct-current power source 105 such that electrons can flow from the anode 103 back to the source 105.
  • the source of current 105 can be configured such that a potential difference is applied across each cathode-anode pair.
  • FIG. 2 A schematic illustration of an electrode 1010/ 103 is shown in FIG. 2.
  • the electrode 101/ 103 is clamped via a fastening mechanism (e.g., a pair of screws) 135 between a pair of electrically conductive plates 133.
  • a voltage is transported from the power source 105 to the electrode 101/103 via an electrically conductive wire 137.
  • one or more of the electrodes 101/103 can be consumable, such that during an advanced oxidation reaction, at least a portion of the electrode 101/ 103 is consumed.
  • a portion of an electrode 101/ 103 can comprise a transition metal that is oxidized and removed from the electrode 101/103.
  • one or more of the electrodes 101/ 013 can be permanent, such that the electrode 101/ 103 is not substantially consumed during an advanced oxidation reaction.
  • the one or more electrodes 101/ 103 can be of any suitable configuration.
  • at least one of the electrodes 101/ 103 can be flat and of a shape suitable for transmitting electrons between a current source 105 and a liquid medium (e.g., a liquid bath contained in a reactor vessel 107).
  • a liquid medium e.g., a liquid bath contained in a reactor vessel 107.
  • at least one of the electrodes 101/ 103 can be rectangular, circular, or triangular, or of any other flat shape.
  • the electrodes 101 and 103 are arranged in a parallel configuration, such that the largest face of each electrode 101/ 103 is parallel to that of each other electrode 101/ 103; and the spacings between each electrode 101/ 103 to each of its nearest and next -nearest neighbors are approximately equal.
  • the one or more electrodes 101/103 are configured to rotate around an axis.
  • the one or more electrodes 101/ 103 are partially submerged in the liquid medium such that, as they rotate, a portion of the electrode 101/103 can become submerged and another portion of the electrode can emerge. Without wishing to be bound to a particular theory, it is believed that rotating a partially submerged electrode 101/ 103 can expose the electrode 101/ 103 to gasses that facilitate an advanced oxidation reaction.
  • the one or more electrodes 101/103 are tubular. In some exemplifications including tubular electrodes, the electrodes 101 and 103 are arranged concentrically such that the axis of each electrode 101/ 103 is aligned, and the electrodes 101 and 103 are centered about this common axis.
  • the anode 103 can comprise any suitable conductive material.
  • the anode can be formed of platinum or can be platinum-coated.
  • the anode 103 can comprise iron.
  • the anode 103 can be configured such that at least a portion of the anode 103 is consumed during an advanced oxidation reaction.
  • the advanced oxidation reactor 100 can alternatively include a plurality of anodes 103.
  • each anode 103 can be identical; or, alternatively, different anodes 103 can be used.
  • the cathode 101 of the advanced oxidation reactor 100 comprises a transition- metal foam.
  • a transition-metal foam comprises a transition metal in a cellular structure with a high porosity.
  • the transition-metal foam comprises an open-cell structure such that the pores are interconnected.
  • Such a structure can have a specific surface area that can increase the available cathode interface for electrochemical reactions.
  • the advanced oxidation reactor 100 can alternatively include a plurality of cathodes 101.
  • the advanced oxidation reactor 100 can include an array of cathodes 101 electrically connected in parallel. Each cathode 101 can be identical; alternatively, different cathodes 101 can be used.
  • the transition metal of the transition-metal foam can be nickel, iron, aluminum, rubidium, cobalt, chromium, copper, manganese, cerium, alloys comprising any of the above, or any other transition metal or alloy. As is described in further detail, infra, we discovered that transition metals enhance the production of hydroxyl radicals from hydrogen peroxide and/ or oxygen; and that effect may be considered to be unexpected.
  • the cathode 101 of the advanced oxidation reactor 100 additionally comprises a carbon coating.
  • the cathode can be constructed by, for example, coating a transition- metal foam (e.g., nickel foam) with a form of carbon [e.g., three-dimensional (3D) graphene].
  • the coating can comprise graphene (e.g., 3D graphene), carbon nanotubes, or any other carbon structure suitable for the transmission of electrons.
  • the carbon coating can be a 3D structure, for example, 3D graphene.
  • a 3D carbon structure is differentiated from 2D graphene structures (e.g., monolayer graphene or multi-layer graphene deposited on a flat substrate) by features of its surface that are observable under an electron microscope. While 2D graphene structures typically comprise one or more flat and parallel-oriented layers, 3D graphene is highly porous. 3D carbon coatings, when used in combination with a metal foam substrate, can greatly enhance the already high surface area of the substrate.
  • 3D graphene coating may not have some of the beneficial electrochemical properties of monolayer graphene (e.g., an absence of inter-sheet junction contact resistance), it has been found that these shortcomings can be overcome by surface-area enhancement of the 3D-graphene coating of a transition-metal foam.
  • the carbon coating is highly conductive. Without wishing to be bound to a particular theory, it is believed that a highly conductive carbon coating can increase the rate of hydrogen peroxide formation.
  • the conductivity of the carbon coating is at least 330 Siemens per meter (S/m). In certain exemplifications, the conductivity of the carbon coating is at least 200 kS/m. In some exemplifications, the cathode 101 has a high specific surface area.
  • Specific surface area is defined to mean the total surface area of a solid, divided by the mass of the solid. Without wishing to be bound to a particular theory, it is believed that a high specific surface area can increase the rate of electrons available from the cathode 101 for electrode chemical reactions.
  • the specific surface area of the cathode 101 can be, e.g., at least 30 m 2 /g. According to some exemplifications, the specific surface area of the cathode 101 is at least 90 m 2 /g.
  • the one or more electrodes is/are disposed within a reactor vessel.
  • a cathode 101 and an anode 103 are disposed within a reactor vessel 107.
  • the reactor vessel 107 can include a first gas inlet 125.
  • the reactor vessel 107 can also include a second gas inlet.
  • the reactor vessel 107 includes a first gas inlet 125 and a second gas inlet 127.
  • the reactor vessel 107 can include only one gas inlet 125/ 127.
  • the reactor vessel 107 also includes a liquid inlet 111.
  • the reactor vessel 107 further includes a liquid outlet 113.
  • the reactor vessel 107 can be of any suitable shape.
  • the reactor vessel 107 can be cylindrical, rectangular, parallelepiped, or conical or can have any other shape suitable for containing a liquid.
  • the reactor vessel 107 can include a flat bottom, a conical bottom, a pyramidal bottom, or a rounded bottom.
  • the reactor vessel 107 includes an open top.
  • the reactor vessel 107 can include a closed top and can also include a gas outlet.
  • the material of the reactor vessel 107 can be non-reactive.
  • suitable materials for forming the reactor vessel 107 include plastics, such as polyethylene terephthalate (PET), high-density polyethylene (HDPE), low-density polyethylene (LDPE), cross-linked polyethylene, linear polyethylene, polypropylene (PP), polyvinyl chloride (PVC), polystyrene (PS), and/or polytetrafluorethylene (PTFE, commercially available as TEFLON fluoropolymer from The Chemours Company.
  • PET polyethylene terephthalate
  • HDPE high-density polyethylene
  • LDPE low-density polyethylene
  • PP polypropylene
  • PVC polyvinyl chloride
  • PS polystyrene
  • PTFE polytetrafluorethylene
  • the reactor vessel 107 can be constructed of, e.g., metal, such as stainless steel, aluminum, or carbon steel, and coated with a non-reactive material, such as
  • the first gas inlet of the reactor vessel 107 can be fluidically connected to a first source of gas 128.
  • the first source of gas 128 is fluidically connected to the first gas inlet 125.
  • the first source of gas 128 can be, e.g., an oxygen source.
  • the oxygen source can comprise pure oxygen (e.g., a pressurized oxygen-filled cylinder) or a mixture of gases, including oxygen, such as air.
  • the first source of gas 128 is an oxygen concentrator.
  • the oxygen source 128 further comprises ozone.
  • the oxygen source 128 can be an oxygen cylinder fluidically connected to an ozone generator.
  • the second gas inlet 127 can be fluidically connected to a second source of gas 129.
  • a second source 129 is fluidically connected to the second gas inlet 127.
  • the second source of gas can comprise ozone.
  • the second source of gas 129 can be an ozone generator.
  • the ozone generator can be an electronic ozone generator fluidically connected to a source of oxygen and configured to produce ozone, for example, by combining oxygen molecules with oxygen radicals produced by rupturing stable oxygen molecules via contact with a corona discharge.
  • a source of oxygen 128 can be fluidically connected to both the ozone generator 129 and the first gas inlet 125.
  • One or more control valves can be fluidically connected to each of the first and/or second gas inlets 125/127.
  • the one or more control valves can control the flow and/or pressure of gas from the first and/or second source of gas 128/129 to the first and/ or second gas inlets 125/ 127, respectively.
  • the control valves can be of any type suitable for controlling flow and/ or pressure.
  • the one or more valves can include one or more ball valves, needle valves, butterfly valves, pressure regulators, and/ or any other suitable type of valves.
  • the first and/ or second gas inlets 125/127 can each be fluidically connected to just a single control valve.
  • first and second gas inlets 125 and 127 can each be fluidically connected to a ball valve.
  • first and/ or second gas inlets 125/ 127 can each be fluidically connected to two or more valves.
  • the first gas inlet 125 can be fluidically connected to a pressure regulator, a ball valve, and a needle valve.
  • the reactor vessel 107 can also include one or more first gas-measurement instruments.
  • the one or more first gas measurement instruments can include, e.g., a flow-measurement instrument, a pressure-measurement instrument, and/or a gas- concentration-measurement instrument.
  • the one or more instruments can be fixed to a conduit that fluidically connects the first and/or second source of gas 128/129 to the first and/or second gas inlets 125 / 127, respectively.
  • at least one of the instruments can be located inside the reactor vessel 107 or within the first and/ or second source of gas 128 / 129.
  • At least one bubble generator 121/ 123 can be disposed within the reactor vessel 107.
  • the at least one bubble generator 121/ 123 can be fluidically connected to the first and/or second gas inlets 125/127.
  • a first bubble generator 121 is fluidically connected to the first gas inlet 125
  • a second bubble generator 123 is fluidically connected to the second gas inlet 127.
  • At least one of the bubble generators 121/ 123 can be fluidically connected to more than one gas inlet 125 and 127, such that gas can flow from more than one gas inlet 125 and 127 into at least one of the bubble generators 121/ 123.
  • each gas inlet 125 and 127 can be fluidically connected to separate bubble generators 121 and 123.
  • multiple bubble generators 121 and 123 can be fluidically connected to one or more gas inlets 125/127 in a parallel configuration.
  • the bubble generators 121 and 123 can be sparger plates; perforated pipes; bubble caps; or porous materials, such as air stones; or can be of any other configuration suitable for dispersing bubbles of gas into a liquid.
  • the reactor vessel 107 can also be configured to receive a liquid stream.
  • the reactor vessel 107 can include a liquid inlet 111 through which the liquid stream can enter.
  • the liquid inlet 111 is located at the top of the reactor vessel 107.
  • the liquid inlet 111 is located at the bottom of the reactor vessel 107.
  • the liquid inlet 111 is located on a sidewall of the reactor vessel 107.
  • the reactor vessel 107 can also include a liquid outlet.
  • the liquid outlet 113 can be located opposite the liquid inlet 111.
  • the liquid inlet 111 can be located at the bottom of the reactor vessel 107 and the liquid outlet 113 can be located at the top of the reactor vessel 107.
  • the liquid outlet 113 is an overflow weir configured such that, when liquid rises above the height of the overflow weir, it can pass over the top of the weir and flow out of the reactor vessel 107. In such cases, the height of the overflow weir can determine the height of the liquid contained in the reactor vessel 107 during steady-state operation.
  • the reactor vessel 107 includes a gas outlet configured such that gas can flow out of the reactor vessel 107 through the gas outlet.
  • the gas outlet can be fluidically connected to an ozone destructor, wherein the ozone destructor can break down effluent ozone to produce a safe effluent gas that is substantially free of ozone.
  • the reactor 100 can also include an agitator 131 configured to increase the replacement rate of liquid and/or gasses at the interface of the electrodes 101 and 103.
  • the agitator 131 can be of any suitable configuration.
  • the agitator 131 can be a paddle, an impeller, or a magnetic stirrer.
  • the agitator 131 can be combined with another element of the reactor 100, such as one or more of the electrodes 101/ 103.
  • the cathode 101 can be configured to rotate via a connection to the agitator 131.
  • a bubble generator 121/123 can be configured to increase the replacement rate of liquid and/or gasses at the surface of the electrodes 101 and 103.
  • the bubble generator 121/123 can be disposed directly beneath one or more of the electrodes 101/103 such that the generated bubbles pass across the surface of the electrode 101/103, increasing the replacement rate of liquid and/or gasses at the interface.
  • the reactor 100 can be used to perform an advanced oxidation method.
  • the method can include, according to some such exemplifications, oxidizing organic materials with hydroxyl radicals.
  • the hydroxyl radicals can be generated by a reaction of ozone with hydrogen peroxide, which is also known to those skilled in the art as the peroxide reaction.
  • Some exemplifications of the method include the electrical generation of the ozone (e.g., with an ozone generator).
  • the method includes in-situ generation of hydrogen peroxide using a carbon-coated transition-metal-foam electrode.
  • the generation of hydroxyl radicals by reacting ozone with hydrogen peroxide, electrochemically produced in-situ with a cathode is known as an electroperoxone process.
  • the method includes oxidation. Oxidation is characterized by the loss of electrons from a molecule, atom, or ion. Oxidation can result in the breakdown of organic molecules into smaller organic molecules. Further oxidation can produce still-smaller organic molecules until only carbon dioxide, water, and simple inorganic compounds remain.
  • the method can utilize advanced oxidation. Advanced oxidation, as used herein, refers to an oxidation process using hydroxyl radicals as an oxidant.
  • hydroxyl radicals are used to remove electrons from molecules, atoms, or ions, which can result in the breakdown of organic molecules into smaller molecules.
  • Advanced oxidation processes may be more effective than other forms of oxidation. Without wishing to be bound to a particular theory, the greater effectiveness of advanced oxidation may be due to the high oxidation potential of hydroxyl radicals.
  • the oxidation potential of hydroxyl radicals and other oxidants are shown in the table, below.
  • the advanced oxidation method can mineralize one or more or, in some cases, substantially all organics in a wastewater stream.
  • mineralization refers to the complete oxidation of an organic molecule, such that the remnants of the molecule essentially consist of carbon dioxide, water, and simple inorganics.
  • the advanced oxidation method may be nonspecific.
  • the oxidation method maybe capable of oxidizing almost any type of organic molecule.
  • Nonspecific oxidation methods can be particularly beneficial when compared to specific oxidation methods, in which only a specific organic molecule or group of similar organic molecules can be oxidized by the method.
  • Nonspecific oxidation methods can be particularly useful for the mineralization of organic molecules because the process may not result in organic molecules that cannot be further oxidized by the process.
  • the organic molecules oxidized by the method can be a constituent of a feed stream; and the method can include treating the feed stream.
  • the feed stream can further comprise, e.g., hydrocarbons and can originate from a source of oilfield wastewater.
  • the total organic carbon (TOC) due to the presence of hydrocarbons can be relatively high.
  • the TOC due to the presence of hydrocarbons can be at least 1,000 mg/L.
  • the TOC due to the presence of hydrocarbons can be at least 3,000 mg/L.
  • TOC is the concentration of carbon, excluding carbon in the form of inorganic salts, such as carbonic acid or carbon dioxide.
  • TOC can be measured by spectrophotometry, for example, with HACH test #2760445 (Hach Company, Loveland, Colorado, USA) for high TOC ranges or HACH test #2760345 for lower TOC ranges, as appropriate.
  • HACH test #2760445 Haach Company, Loveland, Colorado, USA
  • HACH test #2760345 HACH test #2760345 for lower TOC ranges, as appropriate.
  • the reduction of TOC can be highly dependent on the source of the organics, which are often characterized by the source.
  • the reduction of TOC originating from a landfill leachate source can be significantly slower than the reduction of TOC originating from a hydrocarbon source.
  • it is believed that the slower reduction of TOC from a landfill leachate source may be due to the presence of persistent organic pollutants that are somewhat resistant to oxidation.
  • the feed stream can originate from a source of landfill leachate.
  • the feed stream can contain humic acids.
  • the TOC of a landfill leachate stream can be relatively high.
  • the landfill leachate stream can be at least 500 mg/L.
  • the landfill leachate stream can have a TOC of at least 1,000 mg/L.
  • the source of the feed stream is pharmaceutical wastewater.
  • the feed stream can comprise antibiotics.
  • the TOC of the pharmaceutical wastewater is relatively high.
  • a feed stream comprising pharmaceutical wastewater can have a TOC of at least 50 mg/L or, in additional exemplifications, at least 300 mg/L
  • the feed stream can comprise persistent organic contaminants.
  • persistent organic pollutants refer to organic constituents of a water stream that are not substantially removed by conventional water treatment techniques, such as aerobic and/or anaerobic digestion, ozonation, chlorination, or environmental degradation. Persistent organic pollutants can be harmful to living organisms due to their tendency to bioaccumulate.
  • These persistent organic pollutants in the feed stream can include aldrin, chlordane, dieldrin, endrin, heptachlor, hexachlorobenzene, mirex, toxaphene, polychlorinated biphenyls, dichlorodiphenyltrichloroethane, dioxins, polychlorinated dibenzofurans, chlordecone, a-hexachlorocyclohexane, b-hexachlorocyclohexane, hexabromodiphenyl ether, heptabromodiphenyl ether, lindane, pentachlorobenzene, tetrabromodiphenyl ether, perflourooctanesulfonic acid, endosulfans, and/or hexabromocyclododecane.
  • the advanced oxidation method includes an electroperoxone process.
  • Ozone can be produced from oxygen in situ via an electrically powered ozone generator.
  • An electroperoxone process can be particularly advantageous over other advanced oxidation processes because all of the reactants required in the hydrogen-peroxide reaction can be produced in electrochemical reactions from oxygen, an ingredient readily available from the ambient environment.
  • the required oxygen can be supplied from a pure oxygen source; however, a mixed gas source, such as air, that comprises oxygen may alternatively be used.
  • the method includes the oxidation of organics with hydroxyl radicals.
  • the hydroxyl radicals can be produced in an aqueous solution.
  • the hydroxyl radicals can be formed in a reaction between ozone and aqueous hydrogen peroxide.
  • Some exemplifications include producing a solution comprising hydroxyl radicals with a relatively high indicated activity.
  • the activity of a solution comprising hydroxyl radicals can be measured by an indoxyl-P-glucuronide (IBG) chemiluminescence method. In this measurement method, indoxyl-P-glucuronide (IBG) is exposed to hydroxyl radicals; and its oxidation is allowed to occur, resulting in a luminescent product.
  • IBG indoxyl-P-glucuronide
  • an ultraweak chemiluminescence analyzer for example, a BJL-i-IC ultraweak chemiluminescence analyzer from Jye Horn Co., Taipai, Taiwan
  • a high sensitivity detector is then used to measure the chemiluminescence, resulting in a measurement of relative light units.
  • this measurement method yields relatively high measurements of relative light units.
  • the measured relative light units can be at least 75; at least 1,000; at least 1,250; or, in some cases, at least 1,500.
  • the hydroxyl radicals are produced in a reaction in which ozone is a reactant.
  • the ozone can be produced, in some exemplifications, by an ozone generator fluidically connected to the advanced oxidation reactor.
  • the ozone generator can be of any type suitable for the production of ozone.
  • the ozone generator can include a UV light or an electrical corona- discharge.
  • the ozone-generation method can include flowing a gas comprising oxygen to the ozone generator.
  • the gas comprising oxygen is relatively pure oxygen.
  • the gas comprising oxygen is a gas mixture, such as air.
  • the ozone generated by the ozone generator can be flowed to the advanced oxidation reactor as a component of an ozone-containing stream, according to some exemplifications.
  • the concentration of ozone within the ozone-containing stream can be relatively high.
  • the ozone concentration can be in the range of 10 to 200 mg of ozone per liter of ozone-containing gas.
  • the concentration of ozone in the ozone-containing gas can be between 140 and 180 mg/L.
  • the method includes measuring the concentration of ozone within the ozone-containing gas stream prior to its entry to the advanced oxidation reactor.
  • the concentration of ozone is used to control the production of ozone.
  • the control method can be automated, such as with a process controller programmed with a feedback control program; or, alternatively, the control method can be manual.
  • the concentration measurement can be used to adjust the voltage of the ozone generator, the flow of gas to or from the generator, or any other parameter affecting the rate of ozone delivered to the reactor.
  • the rate of ozone-containing gas flowed to the reactor can be relatively high.
  • the rate of ozone-containing gas per liter of reactor volume can be at least 0.01 L/s, at least 0.025 L/s, at least 0.05 L/s, at least 0.075 L/s, at least 0.1 L/s, or at least 0.125.
  • the hydroxyl radicals are produced in a reaction in which hydrogen peroxide is a reactant.
  • the hydrogen peroxide can be produced, for example, by a two-electron reduction of oxygen occurring within the advanced oxidation reactor.
  • gaseous oxygen and two aqueous protons react to form the hydrogen peroxide, with the additional two electrons being provided by the submerged cathode.
  • the resulting product of the reaction is aqueous hydrogen peroxide.
  • a deleterious four-electron-reduction reaction may also occur.
  • diatomic oxygen undergoes a four-electron reduction enabled by the transmission of electrons from the cathode and combines with aqueous protons to form water.
  • Four- electron reduction is disadvantageous to the advanced oxidation process due to the consumption of oxygen and electrical energy that could otherwise be utilized by the two-electron oxygen reduction or by other oxidant-producing reactions.
  • the use of a carbon-coated, transition-metal foam electrode can increase the amount of two-electron oxygen-reduction reactions while decreasing the amount of four-electron oxygen- reduction reactions.
  • the method includes flowing oxygen to the advanced oxidation reactor.
  • the oxygen can be flowed from an oxygen source, which can provide, e.g., pure oxygen.
  • the source of oxygen can be ambient air.
  • At least a portion of the oxygen flowed from the oxygen source to the advanced oxidation reactor can undergo a two-electron-reduction reaction to form hydrogen peroxide.
  • the oxygen can flow into the reactor at a relatively high rate.
  • the rate of ozone entering the reactor, per liter of reactor volume can be at least o.oi L/s, at least 0.025 L/s, at least 0.05 L/s, at least 0.075 L/s, at least 0.1 L/s, or at least 0.125.
  • the method includes transmitting an electrical current between at least two submerged electrodes.
  • the cathode can supply electrons to drive electrochemical reactions, including two-electron reduction of the supplied oxygen.
  • the electrical current is carefully controlled to optimize the production of hydrogen peroxide and/ or hydroxyl radicals.
  • the current can be controlled such that so-to-6oo mA flow between at least two electrodes.
  • the current can be between 100 and 400 mA.
  • the method can include establishing or controlling an electric potential across at least two electrodes.
  • the electric potential can be carefully controlled to optimize the production of hydrogen peroxide and/or hydroxyl radicals.
  • the electric potential can be between 1 to 10 V, or, in more-particular exemplifications, the electric potential can be between 2 and 6 V.
  • the method can include a superoxide-anion- radical reaction.
  • Diatomic oxygen molecules in contact with the submerged electrode comprising a transition metal can undergo one-electron-reduction reactions to form superoxide anion radicals.
  • At least a portion of the resulting superoxide anion radicals can combine with aqueous protons present in the liquid to form hydrogen peroxide.
  • This process of hydrogen-peroxide production can coincide with the production of additional hydrogen peroxide via two-electron oxygen reduction.
  • the hydrogen peroxide produced from the superoxide anion radical can combine with ozone to form hydroxyl radicals.
  • the presence of this reaction in the electroperoxone process can thus be demonstrated by performing the process in the absence of ozone.
  • the reaction of the transition metal and hydrogen peroxide can be greatly facilitated by using a carbon-coated, transition-metal foam electrode.
  • a carbon-coated, transition-metal foam electrode it is believed that the high surface area and conductivity of the carbon-coating-and-metal-foam structures of such an electrode enhance the production of hydrogen peroxide, while the electrochemical properties of the transition metal allow the formation of hydroxyl radicals from hydrogen peroxide in the reaction of the transition metal and hydrogen peroxide.
  • the high surface area of the transition-metal foam can further promote the reaction of the transition metal and the hydrogen peroxide.
  • the method includes regulating the pH of the advanced oxidation reactor.
  • the pH can be adjusted according to any suitable method.
  • the pH can be adjusted by a controlled addition of an acid (e.g., hydrochloric acid, sulfuric acid, etc.) or a base (e.g., caustic soda, potassium hydroxide, lime, etc.).
  • the pH can be adjusted so that it is, for example, in the range of 3 to 9.
  • the method includes adjusting a temperature within the advanced oxidation reactor.
  • the temperature of a liquid entering the reactor can be adjusted.
  • the temperature of the liquid within the reactor can be adjusted (e.g., heated or cooled).
  • the reactor can include a heat exchanger configured to adjust the temperature of the liquid in the reactor.
  • reducing the temperature of the liquid within the advanced oxidation reactor can enhance the production of hydroxyl radicals.
  • the temperature of the liquid within the reactor can be adjusted such that it is below 40 °C, below 30 °C, or in some cases, below 20 °C, or within a particular range.
  • the temperature of the liquid can be adjusted such that it is within the range of o to 40 °C.
  • the temperature of the liquid can be adjusted such that is within the range of 20 to 30 °C.
  • the residence time of the feed liquid within the advanced oxidation reactor can be relatively large.
  • the reactor vessel is sized to provide a specified residence time.
  • the residence time can be at least 1 hour, at least 2 hours, at least 3 hours, at least 4 hours, at least 5 hours, at least 6 hours, at least 7 hours, at least 8 hours, at least 9 hours, at least 10 hours, at least 11 hours, or in some cases at least 12 hours.
  • the reactor vessel can be designed to provide a residence time within a specified range.
  • the residence time can be between 1 and 2 hours, between 2 and 3 hours, between 3 and 4 hours, between 4 and 5 hours, between 5 and 6 hours, between 6 and 7 hours, between 7 and 8 hours, between 7 and 9 hours, between 8 and 9 hours, between 9 and 10 hours, between 10 and 11 hours, or between 11 and 12 hours.
  • the residence time for which the reactor vessel is designed can be determined based on the source of the feed solution.
  • the residence time can be at least 1 hour, at least 2 hours, at least 3 hours, at least 4 hours, or in some cases, at least 5 hours.
  • the residence time can be within a particular range, such as between 1 and 2 hours, between 2 and 3 hours, between 3 and 4 hours, or in some cases, between 4 and 5 hours when the source of the feed solution is pharmaceutical wastewater.
  • the residence time can be at least 6 hours, at least 7 hours, at least 8 hours, at least 9 hours, at least 10 hours, at least 11 hours, or in some cases at least 12 hours.
  • the reactor vessel can be designed to provide a residence time within a particular range, such as between 6 and 7 hours, between 7 and 8 hours, between 7 and 9 hours, between 8 and 9 hours, between 9 and 10 hours, between 10 and 11 hours, or in some cases between 11 and 12 hours when the source of the feed solution is landfill leachate.
  • the residence time can be at least 6 hours, at least 7 hours, at least 8 hours, at least 9 hours, at least 10 hours, at least 11 hours, or in some cases at least 12 hours.
  • the reactor vessel can be designed to provide a residence time within a particular range, such as between 6 and 7 hours, between 7 and 8 hours, between 7 and 9 hours, between 8 and 9 hours, between 9 and 10 hours, between 10 and 11 hours, or in some cases between 11 and 12 hours when the source of the feed solution is oilfield wastewater.
  • the residence time is calculated by dividing the flow rate of liquid into a reactor vessel by the volume of the reactor vessel.
  • the residence time corresponds to the amount of time a volume of liquid spends in the reactor vessel.
  • the residence time is equivalent to the average amount of time that liquid spends within the reactor vessel. A large amount of TOC can be removed by the advanced oxidation process.
  • the reduction of TOC from the feed solution can be at least 1 mg/L, at least 4 mg/L, at 7 least mg/L, or at 10 least mg/L. According to other exemplifications, the reduction of TOC from the feed solution can be at least 50 mg/L, at least 100 mg/L, at least 500 mg/L, or in some cases at least 1,000 mg/L. In some exemplifications, a relatively high percentage of the TOC within the feed stream can be removed; for example, at least 75% of the TOC can be removed.
  • the TOC of the feed stream is reduced by at least 80%, at least 90%, at least 95%, or at least 99%; and, in some exemplifications, substantially no TOC is left after the process is complete.
  • a relatively large amount of color can be removed from the feed stream by the advanced oxidation process.
  • the true color of water differs from its apparent color in that true color is measured after all suspended particulate matter has been removed.
  • a relatively high percentage of the true color can be removed; for example, the percentage of true color removed can be at least 90%, at least 95%, or at least 99%; and, in some exemplifications, substantially all of the true color is removed.
  • a relatively high percentage of apparent color is removed.
  • the percentage of apparent color removed can be at least 80%, at least 85%, at least 90%, at least 95%, or at least 99%; and, in some exemplifications, substantially all of the apparent color is removed.
  • the advanced oxidation method can remove a relatively large amount of persistent organic pollutants from the feed stream.
  • relatively high percentages of the mass concentration of persistent organic pollutants are removed.
  • the percentage of persistent organic pollutants removed from the feed stream can be at least 90%, at least 95%, or at least 99%; and, in some exemplifications, substantially all the persistent organic pollutants are removed from the feed stream.
  • the advanced oxidation method can remove a relatively large amount of cellular adenosine triphosphate (cATP) from the feed stream.
  • cATP cellular adenosine triphosphate
  • cATP is associated with living organisms in a water sample; and, thus, the measurement of cATP serves as a proxy for the measurement of microbial content (e.g., bacteria).
  • cATP is typically measured using a procedure including the use of a luminometer (e.g., the PHOTONMASTER luminometer manufactured by
  • LuminUltra Technologies, Ltd. of Fredricton, New Brunswick, Canada
  • a single-point calibration step is performed by reacting a known concentration of cATP with an enzyme reagent constraining luciferase (e.g., LUMINASE reagent, manufactured by LuminUltra Technologies, Ltd.) and measuring the resulting light produced in the luminometer measure in relative light units (RLU), expressed as RLUATPI in Equation 1, below.
  • RLU relative light units
  • Non-mi crobial content is washed from the filter using a cleaning solution (e.g., LUMICLEAN solution manufactured by LuminUltra Technologies, Ltd.), and excess moisture is removed by forcing air through the filter.
  • An ATP extraction reagent e.g., ULTRALYSE 7 reagent manufactured by LuminUltra Technologies, Ltd
  • a dilution reagent e.g., ULTRALUTE reagent manufactured by LuminUltra
  • cATP in the feed stream can be removed.
  • the percentage of cATP removed from the feed stream can be at least 90%, at least 95%, or at least 99%; and, in some exemplifications, substantially all of the cATP is removed.
  • the advanced oxidation process is the electrofenton process.
  • the electrofenton process includes the oxidation of an iron catalyst with cathodically generated hydrogen peroxide to produce hydroxyl radicals.
  • a carbon-coated, transition- metal foam electrode is particularly beneficial to such a process due to such an electrode's superior ability to produce hydrogen peroxide.
  • the advanced oxidation process includes photoelectrocatalysis.
  • Photoelectrocatalysis involves the formation of hydroxyl radicals via oxidation of water and hydroxyl ions by holes produced from the photo-excitation of a semiconductor to create electron/hole pairs in conjunction with the separation of the produced electron/hole pairs by an anodic bias applied to the semiconductor. Because the generation of hydroxyl radicals in photoelectrocatalysis occurs due to electrochemical reactions at the anode, photoelectrocatalysis can be practiced in combination with electroperoxone, where the production of hydroxyl radicals occurs due to electrochemical reactions at the cathode. Furthermore, the operational parameters, such as electrode spacing, current, pH, and potential difference across the electrodes that are beneficial for electroperoxone are also beneficial for photoelectrocatalysis.
  • the advanced oxidation process is performed as part of a larger water-treatment -process train.
  • aerobic and/ or aerobic digestion can be performed on the feed stream prior to the advanced oxidation process. Upstream aerobic and/ or anaerobic digestion can remove more-easily oxidizable organic material in an energy-efficient way.
  • a polishing step can be performed after the advanced oxidation process. The polishing step can include the use of granular activated carbon (GAC).
  • GAC granular activated carbon
  • an advanced-oxidation-process effluent stream comprising liquid treated by the advanced oxidation process and having a lower TOC content as compared to the feed liquid, can be flowed to a vessel containing GAC, where at least a portion of the remaining TOC is adsorbed to the GAC.
  • the larger water treatment process train includes the use of a recirculation loop via which at least a portion of the effluent exiting one treatment step (e.g., digestion, the advanced oxidation process, and/or the polishing step) is directed back to a previous treatment step.
  • a portion of liquid exiting the advanced oxidation process can be directed back to be treated in the aerobic and/ or anaerobic digestion step.
  • a reference to "A and/or B,” when used in conjunction with open-ended language such as “comprising” can refer, in one embodiment, to A without B (optionally including elements other than B); in another embodiment, to B without A (optionally including elements other than A); and, in yet another embodiment, to both A and B (optionally including other elements); etc.
  • the phrase "at least one,” in reference to a list of one or more elements, should be understood to mean at least one element selected from any one or more of the elements in the list of elements, but not necessarily including at least one of each and every element specifically listed within the list of elements and not excluding any combinations of elements in the list of elements.
  • This definition also allows for additional elements to optionally be present other than the elements specifically identified within the list of elements to which the phrase, "at least one,” refers, whether related or unrelated to those elements specifically identified.
  • At least one of A and B can refer, in one embodiment, to at least one, optionally including more than one, A, with no B present (and optionally including elements other than B); in another embodiment, to at least one, optionally including more than one, B, with no A present (and optionally including elements other than A); in yet another embodiment, to at least one, optionally including more than one, A, and at least one, optionally including more than one, B (and optionally including other elements); etc.
  • the word “purified” (and, similarly, “pure” and “purify”) is used to describe any liquid that contains the component of interest in a higher percentage than is contained within a reference stream, and does not necessarily require that the liquid is 100% pure. That is to say, a “purified” stream can be partially or completely purified. As a non-limiting example, a water stream may be made up of 80 wt% water but could still be considered “purified” relative to a feed stream that is made up of 50 wt% water. Of course, it should also be understood that, in some embodiments, the "purified” stream could be made up of only (or substantially only) the component of interest.
  • a "purified" water stream could be made up of substantially only water (e.g., water in an amount of at least 98 wt%, at least 99 wt%, or at least 99.9 wt%) and/or could be made up of only water (i.e., 100 wt% water).
  • Electric connections may include permanent electrical connections (e.g., soldered connections) and/or temporary electrical connections (e.g., screw terminal connections, plug and socket connections).
  • permanent electrical connections e.g., soldered connections
  • temporary electrical connections e.g., screw terminal connections, plug and socket connections
  • an electrical connection exists when electrons may be allowed to flow from one device or system to another electrically connected device or system.
  • Electrical connections may further be switchable, as provided, e.g., by switches, relays, fuses, or other devices capable of interrupting or controlling the flow of electricity through the electrical connection.
  • Fluidic connections maybe either direct fluidic connections or indirect fluidic connections.
  • a direct fluidic connection exists between a first region and a second region (and the two regions are said to be directly fluidically connected to each other) when they are fluidically connected to each other and when the composition of the fluid at the second region of the fluidic connection has not substantially changed relative to the composition of the fluid at the first region of the fluidic connection (i.e., no fluid component that was present in the first region of the fluidic connection is present in a weight percentage in the second region of the fluidic connection that is more than 5% different from the weight percentage of that component in the first region of the fluidic connection).
  • a stream that connects first and second unit operations, and in which the fluid's pressure and temperature are adjusted but the composition of the fluid is not altered would be said to directly fluidically connect the first and second unit operations. If, on the other hand, a separation step is performed and/or a chemical reaction is performed that substantially alters the composition of the stream contents during its passage from the first component to the second component, the stream would not be said to directly fluidically connect the first- and second-unit operations.
  • a direct fluidic connection between a first region and a second region can be configured such that the fluid does not undergo a phase change from the first region to the second region.
  • the direct fluidic connection can be configured such that at least 50 wt% (or at least 75 wt%, at least 90 wt%, at least 95 wt%, or at least 98 wt%) of the fluid in the first region is transported to the second region via the direct fluidic connection.
  • Any of the fluidic connections described herein maybe, in some exemplifications, direct fluidic connections. In other cases, the fluidic connections may be indirect fluidic connections.
  • those parameters or values can be adjusted up or down by 1/ 100 th , 1/ 50 th , 1/ 20 th , 1/ 10 th , 1/ 5 th , 173 rd , 1/2, 2/3 rd , 3/4*, 4/5*, 9/io th , 19/20*, 49/50*, 99/100*, etc.
  • a cathode for an advanced oxidation reactor wherein the cathode comprises: a transition-metal foam; and a carbon coating on the transition-metal foam.
  • An advanced oxidation reactor comprising: the cathode of any one of the preceding clauses; and an anode configured and positioned with respect to the cathode such that a potential difference can be applied across the anode and the cathode.
  • reactor vessel further comprises a liquid inlet fluidically connected to a source of feed liquid and configured to receive a feed liquid stream from the source of feed liquid.
  • the reactor of clause 19 further comprising a flow controller configured to receive an electrical signal from the first total-organic-carbon sensor and to control the residence time of a liquid within the reactor vessel in response to the electrical signal.
  • 21 The advanced oxidation reactor of clause 20, further comprising a second total- organic-carbon sensor configured to detect a concentration of total organic carbon in a feed liquid entering the reactor vessel.
  • An advanced oxidation method comprising; electrifying a cathode comprising a transition-metal foam and a carbon coating on the transition-metal foam to produce an electrified cathode; using the electrified cathode to produce a hydrogen-peroxide product via a first electrochemical reaction; producing OH radicals via a second electrochemical reaction involving the hydrogen peroxide product; and oxidizing organic molecules from a feed stream using the OH radicals.
  • An electroperoxone method comprising: providing a cathode and an anode, electrically connectable to a source of direct current, wherein the cathode and anode are at least partially submerged in a liquid bath comprising a feed solution in a reactor vessel; injecting a gas stream comprising ozone into the liquid bath; injecting a gas stream comprising oxygen into the liquid bath; and transmitting a current from the cathode to the anode, resulting in an electrochemical reaction in which hydroxyl radicals are produced, wherein organic chemicals contained in the liquid bath are oxidized by the hydroxyl radicals, and wherein the cathode comprises carbon-coated nickel foam.

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Abstract

Selon l'invention, une cathode, qui peut être utilisée en combinaison avec une anode dans un réacteur d'oxydation avancée, comprend une mousse de métal de transition et un revêtement de carbone sur la mousse de métal de transition. L'oxydation peut être réalisée par électrification de la cathode et utilisation de la cathode électrifiée pour produire un produit de peroxyde d'hydrogène par l'intermédiaire d'une première réaction électrochimique. Des radicaux OH peuvent être produits par l'intermédiaire d'une seconde réaction électrochimique impliquant le produit de peroxyde d'hydrogène. Des molécules organiques peuvent ensuite être oxydées à partir d'un courant d'alimentation à l'aide des radicaux OH.
PCT/US2021/021739 2020-03-10 2021-03-10 Électrodes de métal de transition revêtues de carbone pour réacteurs d'oxydation avancée WO2021211231A2 (fr)

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CN115520943A (zh) * 2022-09-29 2022-12-27 四川大学 以臭氧扩散电极为阳极电催化臭氧处理医院污水的方法
CN115739153A (zh) * 2022-11-10 2023-03-07 湖南大学 一种直接催化电化学还原氧气为羟基自由基的催化剂及其制备方法和应用
SE2251224A1 (en) * 2022-10-19 2024-04-20 Chemox I Umeaa Ab Water purification involving an electro-peroxone process

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DE102013011395A1 (de) * 2013-07-03 2015-01-08 H2O-TecSystems UG (haftungsbeschränkt) Verfahren zur Abwasserbehandlung und Einrichtung zur Durchführung dieses Verfahrens
EP3145875B1 (fr) * 2014-05-23 2021-09-22 Hydrus Technology Pty. Ltd. Procédé de traitement électrochimique
GB2554606B (en) * 2015-05-07 2021-08-11 Evoqua Water Tech Llc Advanced oxidation process methods for degasification of reactor vessel
CN108203141A (zh) * 2016-12-19 2018-06-26 哈尔滨皓威伟业科技发展有限公司 一种滤过式电极电解制双氧水的预氧化方法
CN110143647B (zh) * 2019-05-22 2022-01-07 北京工业大学 一种碳纳米管-nafion/泡沫金属气体扩散电极的制备方法与应用

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115520943A (zh) * 2022-09-29 2022-12-27 四川大学 以臭氧扩散电极为阳极电催化臭氧处理医院污水的方法
CN115520943B (zh) * 2022-09-29 2024-03-01 四川大学 以臭氧扩散电极为阳极电催化臭氧处理医院污水的方法
SE2251224A1 (en) * 2022-10-19 2024-04-20 Chemox I Umeaa Ab Water purification involving an electro-peroxone process
CN115739153A (zh) * 2022-11-10 2023-03-07 湖南大学 一种直接催化电化学还原氧气为羟基自由基的催化剂及其制备方法和应用

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